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橡胶及橡胶制品中4种酚类防霉剂的高效液相色谱法测定
引用本文:王卉卉,叶曦雯,于世涛,牛增元,李静,李晶莹,钱翌.橡胶及橡胶制品中4种酚类防霉剂的高效液相色谱法测定[J].分析测试学报,2010,29(3).
作者姓名:王卉卉  叶曦雯  于世涛  牛增元  李静  李晶莹  钱翌
作者单位:1. 青岛科技大学,环境与安全工程学院,山东,青岛,266042
2. 山东出入境检验检疫局,山东,青岛,266002
基金项目:国家质检公益性行业科研专项基金资助项目 
摘    要:建立了橡胶及其制品中硝基苯酚(PNP)、2,3,5,6-四氯苯酚(TeCP)、五氯苯酚(PCP)、邻苯基苯酚(OPP)4种酚类防腐剂的高效液相色谱测定方法。样品冷冻粉碎后,经甲醇超声提取,在Venusil-XBP C18色谱柱(250 mm×4.6 mm,5μm)上以10 mmol/L醋酸铵和甲醇为流动相梯度洗脱,采用二极管阵列检测器,PCP、TeCP、OPP的检测波长为220 nm,PNP的检测波长为320 nm。4种酚类防霉剂的质量浓度在0.5~250mg/L范围内与峰面积呈良好的线性关系,相关系数大于0.999 4。丁苯橡胶、硅橡胶基体的加标回收实验结果表明:TeCP、PCP、OPP、PNP在不同基质中的平均加标回收率分别为82%~95%、68%~90%、85%~98%、87%~98%,相对标准偏差小于5%。

关 键 词:酚类防腐剂  橡胶  硝基苯酚  2  3  5  6-四氯苯酚  五氯苯酚  邻苯基苯酚  高效液相色谱

Determination of Four Phenolic Antiseptics in Rubber and Rubber Products by High Performance Liquid Chromatography
WANG Hui-hui,YE Xi-wen,YU Shi-tao,NIU Zeng-yuan,LI Jing,LI Jing-ying,QIAN Yi.Determination of Four Phenolic Antiseptics in Rubber and Rubber Products by High Performance Liquid Chromatography[J].Journal of Instrumental Analysis,2010,29(3).
Authors:WANG Hui-hui  YE Xi-wen  YU Shi-tao  NIU Zeng-yuan  LI Jing  LI Jing-ying  QIAN Yi
Institution:WANG Hui-hui1,YE Xi-wen2,YU Shi-tao1,NIU Zeng-yuan2,LI Jing2,LI Jing-ying1,QIAN Yi1(1.School of Environment , Safety Engineering,Qingdao University of Science , Technology,Qingdao 266042,China,2.Sh,ong Entry-Exit Inspection , Quarantine Bureau,Qingdao 266002,China)
Abstract:A high performance liquid chromatographic(HPLC) method was developed for the determination of four phenolic antiseptics,including nitrophenol(PNP),2,3,5,6-tetrachlorophenol(TeCP),pentachlorophenol(PCP),o-phenylphenol(OPP) in rubber and rubber products.After freeze grinding,the samples were ultrasonicly extracted with methanol.The separation and quantification of four phenolic antiseptics were achieved by an Venusil-XBP C_(18)(250 mm×4.6 mm,5 μm) using a mixture of 10 mmol/L NH4Ac and methanol as the mobile phase and detecting with diode array detector(DAD) at 220 nm for PCP,TeCP,OPP,and 320 nm for PNP.There were good linear relationship between the chromatographic peak areas and the concentrations of four phenolic antiseptics in the range of 0.5-250 mg/L with correlation coefficients more than 0.999 4.The recoveries of spiked samples in different matrix were 82% -95% for TeCP,68% -90% for PCP,85% -98% for OPP and 87% -98% for PNP,respectively.The relative standard deviations(n=6) were lower than 5%.The results showed that the method was simple,rapid and accurate,and was successfully applied in the analysis of phenolic antiseptics in rubber and rubber products.
Keywords:phenolic antiseptics  rubber  nitrophenol  2  3  5  6-tetrachloro-phenol  pentachlorophenol  o-phenylphenol  high performance liquid chromatography(HPLC)
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